液相色谱串联质谱法测定水产品中的敌百虫残留量

Determination of Trichlorfon Residue in Aquatic Products by Liquid Chromatography-Mass Spectrometry

将水产品样品经乙腈提取,正已烷除脂,旋转浓缩后采用液相色谱串联质谱法进行定性、定量分析。线性范围为5—100μg/kg,线性相关系数为0.9987,定性检出限1.7μg/kg,定量检出限3.5μg/kg。在鳗鱼、虾和罗非鱼3种不同样品基质中进行添加浓度为10,20,50μg/kg的验证实验,回收率在77.2%—87.5%之间,相对标准偏差(RSD)在5.4%—8.3%之间,并对敌百虫的质谱裂解进行了分析。本法快速简单,高效,灵敏度高,符合检测要求。

The compound was extracted with acetonitrile and cleaned with hexane,and concentrated with rotary evaporation.The treated sample solution was qualitatively and quantitatively analyzed by high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS）.The linear range was between 5 and 100μg/kg with coefficient correlation of 0.9987,and the detection limit was 1.7μg/kg with the quantification limit of 3.5μg/kg.The demonstration test was carried out in different samples（such as eel,shrimp and tilapia fish） at additional concentration of 10,20,50μg/kg,and the recoveries were in the range of 77.2%—87.5%,and RSD were from 5.4% to 8.3%,then the MS fragmentation mechanism of this compound was analyzed.The method is effective,fast and high sensitivity,and that meets the request of detection.